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Heats of Adsorption of N-Hexane by Thermal Gravimetry with Differential Scanning Calorimetry (Tg-DSC): A Tool for Textural Characterization of Pillared Clays

Published online by Cambridge University Press:  28 February 2024

J. Pires ,
M. Brotas de Cavalho ,
A. P. Carvalho ,
J. M. Guil  and
J. A. Perdigón-Melón
J. Pires*
Affiliation:
Departamento de Química e Bioquímica da Faculdade de Ciências de Lisboa, R. Ernesto Vasconcelos, Ed. C1, 5° piso, 1749-016 Lisboa, Portugal
M. Brotas de Cavalho
Affiliation:
Departamento de Química e Bioquímica da Faculdade de Ciências de Lisboa, R. Ernesto Vasconcelos, Ed. C1, 5° piso, 1749-016 Lisboa, Portugal
A. P. Carvalho
Affiliation:
Departamento de Química e Bioquímica da Faculdade de Ciências de Lisboa, R. Ernesto Vasconcelos, Ed. C1, 5° piso, 1749-016 Lisboa, Portugal
J. M. Guil
Affiliation:
Instituto de Química Física “Rocasolano”, CSIC, Serrano 119, 28006 - Madrid, Spain
J. A. Perdigón-Melón
Affiliation:
Instituto de Química Física “Rocasolano”, CSIC, Serrano 119, 28006 - Madrid, Spain
*
E-mail of corresponding author: [email protected]
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Abstract

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Microporous materials, (materials with pore sizes with widths <2 nm) were prepared by pillaring of smectites obtained from different soil deposits. The materials were prepared by intercalation with oligomeric cations of aluminum, which were transformed to aluminum-oxide pillars by calcination. The adsorption of n-hexane in the pillared clays was studied by the determination of heats of adsorption. Heats of adsorption were measured using either a static microcalorimeter or differential scanning calorim-etry coupled with thermogravimetry (TG-DSC). In this latter case, two different procedures were used that differ on the introduction of the (n-hexane) molecules that are to be adsorbed. The results obtained by the (standard) static microcalorimeter method and the TG-DSC method were compared. This comparison showed the heats of adsorption obtained by TG-DSC are differential heats of adsorption, and it showed the range of adsorption. Characterizing the texture of pillared clays, especially microporosity, is important for monitoring the intercalation process and for determining potential applications of these materials. Correlations between the obtained heats of adsorption and the dimensions of micropores suggest that TG-DSC is a semi-quantitative method for characterizing micropores in aluminum-pillared clays.

Keywords

AdsorptionCalorimetryMicroporous MaterialsPillared ClaysTextural CharacterizationTG-DSC
Type
Research Article
Information
Clays and Clay Minerals , Volume 48 , Issue 3 , June 2000 , pp. 385 - 391
Copyright
Copyright © 2000, The Clay Minerals Society

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